WO2004009233A1 - Catalyseur a base solide nanometrique magnetique et son procede de preparation - Google Patents

Catalyseur a base solide nanometrique magnetique et son procede de preparation Download PDF

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Publication number
WO2004009233A1
WO2004009233A1 PCT/CN2003/000592 CN0300592W WO2004009233A1 WO 2004009233 A1 WO2004009233 A1 WO 2004009233A1 CN 0300592 W CN0300592 W CN 0300592W WO 2004009233 A1 WO2004009233 A1 WO 2004009233A1
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WIPO (PCT)
Prior art keywords
magnetic
catalyst
mixed
salt
solution
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PCT/CN2003/000592
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English (en)
Chinese (zh)
Inventor
Xue Duan
Hui Zhang
Rong Qi
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Beijing University Of Chemical Technology
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Publication date
Application filed by Beijing University Of Chemical Technology filed Critical Beijing University Of Chemical Technology
Priority to AU2003255081A priority Critical patent/AU2003255081A1/en
Publication of WO2004009233A1 publication Critical patent/WO2004009233A1/fr
Priority to US11/040,408 priority patent/US7247598B2/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/007—Mixed salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
    • B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/33—Electric or magnetic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0027—Powdering
    • B01J37/0036—Grinding

Definitions

  • the invention relates to a magnetic nano solid base catalyst and a preparation method thereof.
  • heterogeneous catalysis In the field of catalytic research, homogeneous catalysis has gradually transitioned to heterogeneous catalysis.
  • the use of solid bases instead of liquid bases for catalysis has the following advantages: (1) high activity, high selectivity, and high product purity; (2) the catalyst is easy to separate (3) less corrosive to equipment, less waste liquid generated, and reduce environmental pollution.
  • heterogeneous catalysis systems often have disadvantages such as small reaction interface and large mass transfer resistance, which make the catalytic performance significantly lower than that of homogeneous systems, or cannot be widely used for other reasons.
  • Hydrotalcite (LDH) compounds have shown good application prospects in the field of heterogeneous catalysis.
  • LDH Hydrotalcite
  • the nano-sized composite metal oxide particles are extremely small in size, have a large specific surface area, can be in full contact with the substrate, achieve efficient catalytic activity, and have good thermal stability.
  • the disadvantage is that the dispersion in the liquid-solid catalyst system is poor, and it is difficult to separate and recover.
  • the catalyst particles are small, resulting in large bed resistance, which brings difficulties to its industrial application.
  • EP0421677A1, EP0421678A1 describe alkaline hydrotalcite and calcined hydrotalcite as solid base catalysts for the synthesis of alcohol ethers.
  • the general formula of hydrotalcite is [M 2+ a N 3+ b (OH) ( 2a + 3b) ] [X ] b , where M is a divalent metal ion, N is a trivalent metal ion, and X is an equivalent anion, which becomes a Mg-Al-0 complex after firing.
  • the invention provides a nano-scale solid alkali catalyst with magnetic properties, that is, a catalyst coated with a solid alkali active component on the outside of a magnetic core.
  • the reaction can be achieved by controlling the intensity and direction of a magnetic field applied by an external magnetic field.
  • the preparation method of the catalyst is to firstly perform a rapid nucleation reaction using a liquid-liquid reaction all-reverse liquid film reactor (see patent application: 00132145.5) to prepare a nano-level magnetic core, and mix the magnetic core with a corresponding salt solution.
  • An all-reverse liquid film reactor is used to perform a rapid nucleation reaction to obtain a hydrotalcite containing a magnetic core.
  • the hydrotalcite is converted to a corresponding solid alkali composite oxide by high-temperature roasting, and the magnetic core is coated in the composite oxide.
  • the chemical formula of the magnetic nano solid base catalyst prepared by the present invention is:
  • M is any one of the divalent metal ions Mg 2+ , Ni 2+ , Zn 2+ , Ca 2+ or Co 2+ , and N is the trivalent metal ion Fe 3+ , V 3+ , Al 3+ or Gr ⁇ any one of them; M is any one of Mg "Cu 2+ , Ba 2 ⁇ Ni 2+ trivalent metal ion, M and M may be the same or different;
  • M, Fe 2 0 4 is a magnetic species
  • MN- (O) is a composite oxide formed by baking the corresponding hydrotalcite, which is coated on M, Fe 2 0 4 .
  • the preparation method of the catalyst is:
  • the soluble inorganic salt of M, and the soluble inorganic salt of ferric iron are formulated into a mixed solution, wherein the molar ratio of M7Fe 3+ is 0.5 2.0, the molar concentration of M is 0.1-2.5M, and the molar concentration of Fe 3+ is 0.2- 5.0M; a mixed alkali solution was prepared with NaOH and Na 2 C0 3 , wherein the molar concentration of NaOH is 0.1-5.0M, and the molar concentration of Na 2 C0 3 is 0.1 ⁇ 4.8M;
  • the above salt solution and alkaline solution are simultaneously poured into an all-reverse liquid film reactor (see patent application 00132145), the rotation speed of the rotor is controlled to be 1000 to 8000 rpm, and the residence time of the materials in the reactor is 1 to 8 minutes, which are dispersed by the liquid separator. After that, mix thoroughly in the gap between the rotor and the stator, discharge to the crystallization kettle through the discharge port, and crystallize at 80 ⁇ 120 ° C for 2 ⁇ 10h at a constant temperature. Repeat suction filtration, washing, and drying. It is dried and calcined at a high temperature of 800 ⁇ 1000 ° C to obtain M, Fe 2 0 4 powder with a particle size range of 20 ⁇ 80nm. The amount of alkali solution should be added so that the PH value of the mixed liquid is 8.5 ⁇ 11.0.
  • a mixed alkali solution was prepared with NaOH and Na 2 CO ⁇ e.
  • the molar concentration of NaOH is 0.1-5.0M, and the molar concentration of Na 2 C0 3 is 0.1-4.8M;
  • the salt solution and the alkaline solution are simultaneously poured into an all-reverse liquid film reactor, and the rotation speed of the rotor is controlled to be 1000 to 8000 rpm, and the residence time of the material in the reactor is 1 to 8 minutes, and the liquid is passed through the gap between the rotor and the stator Mix thoroughly at the place, drain to the crystallization kettle through the discharge port, and crystallize at 80 ⁇ 120 ° C for 4 ⁇ : LOh, repeatedly suction filtration, washing, and drying to obtain hydrotalcite MN- with magnetic core M, Fe 2 0 4 LDH IM, Fe 2 0 4 .
  • the amount of alkali solution should be added so that the PH value of the mixed liquid is 8.5-11.0.
  • MN-LDH / M and Fe204 are calcined at 400 ⁇ 600 ° C for 2 ⁇ 5 hours, and the heating rate is 10 ° C / min, to obtain a magnetic solid base catalyst MN- (O) / M with a particle size range of 30 ⁇ 100nm.
  • the trivalent salt of iron in step (1) may be: Fe 2 (S0 4 ) 3 , Fe Cl 3 ⁇ Fe (N0 3 ) 3 ; M, the salt may be: M, S0 4 , M, C1 2 , Any of M, (N0 3 ) 2 , M, preferably Zn 2+ , Mg 2+ or Ni 2+ .
  • the preparation of magnetic cores and solid base catalysts uses a fully reversed liquid film reactor for rapid nucleation reaction, the reactants can be fully contacted and collided instantaneously, the nucleation reaction is completed instantaneously, and the crystal nuclei are synchronized. Growth, so the resulting magnetic core and solid base catalyst are both nano-sized particles.
  • the particle size of the catalyst is 30 ⁇ 100 nm, and its magnetic properties are as follows: the coercive force He is 120 ⁇ 108A / m, and the specific saturation magnetization is 2 ⁇ 18 A / m.
  • the magnetic precursor MgAl-LDH / MgFe 2 0 4 was calcined in an air atmosphere at 600 ° C. for 2 hours, and the temperature rising rate was 10 ° C./minute to obtain a magnetic solid base catalyst MgAl (0) / MgFe 2 0 4 .
  • the measured grain size of the catalyst is in the range of 30-85 nm, and the maximum grain size is 62 nm.
  • the coercive force He value is 120.0A / m, and the specific saturation magnetization 6 * is 2.1A / m.
  • the gelatinous substance was poured into a crystallization kettle, and was crystallized at a constant temperature of 100 ° C for 6 hours, and then repeatedly filtered with suction and washed to a pH value of 7.
  • the filter cake was dried in an oven for 24 hours to obtain the magnetic precursor ZnAl-LDH / NiFe. 2 0 4 .
  • the magnetic precursor ZnAl-LDH / NiFe 2 0 4 was fired in an air atmosphere at 600 ° C. for 5 hours, and the temperature rising rate was 10. C / min to obtain a magnetic solid base catalyst ZnAl (0) / NiFe 2 0 4 .
  • the measured grain size is in the range of 30 ⁇ 80nm, and the maximum grain size is 58nm.
  • the coercive force He value is 110.5A / m, and the specific saturation magnetization 6 x is 3.5A / m.
  • the mixed solution stayed in the reactor for 2 minutes, and then the obtained slurry was poured into a crystallization kettle, and was crystallized at 100 ° C for 6 hours, and then repeatedly filtered and washed to a pH value of 7, and the filter cake was placed at 70 ° C. After drying in an oven for 24 hours, it was pulverized, and then calcined in an air atmosphere at 900 ° C for 2 hours. The heating rate was 10 ° C / min, and the magnetic core NiFe 2 0 4 was obtained .
  • magnesium-aluminum molar ratio of 4 1, weigh 41,03g Mg (N0 3 ) 2 -6H 2 0 and 15.01g ⁇ 1 ( ⁇ 0 3 ) 3 ⁇ 9 ⁇ 2 0 in 130ml deionized water to form a mixed salt Solution, and at a molar ratio of Mg (N0 3 ) 2 .6H 2 0 / NiFe 2 0 4 to 5.00, add the prepared NiFe 2 0 4 powder to the mixed salt solution, stir and mix uniformly; weigh 12.8 g NaOH and 8.48g Na 2 C0 3 were dissolved in BOml deionized water to prepare a mixed alkali solution; the two solutions were simultaneously poured into the opened all-reverse liquid film reactor.
  • the rotor speed was controlled at 7000 rpm, and the reaction mixture was Remain in the reactor for 2min, then pour the obtained gum into the crystallization kettle, crystallize at 100 ° C for 6h, and then repeat Suction filtration, washing until the pH is equal to 7, and drying the filter cake in an oven for 24 hours to obtain the magnetic precursor MgAl-LD Li iFe 2 0 4 .
  • the magnetic precursor MgAl-LDH / NiFe 2 0 4 was calcined in an air atmosphere at 550 ° C. for 2 hours, and the temperature rising rate was 10 ° C./minute to obtain a magnetic solid base catalyst MgAl (0) / NiFe 2 0 4 .
  • the measured grain size is in the range of 35 ⁇ 90nm.
  • the maximum grain size is 65nm.
  • the coercive force He value was 130.2 A / m, and the specific saturation magnetization 6 x was 2.6 A / m.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Catalysts (AREA)

Abstract

L'invention concerne un catalyseur à base solide nanométrique magnétique et son procédé de préparation. Le noyau magnétique du catalyseur est enveloppé dans un composant actif à base solide. On met d'abord en oeuvre le procédé selon lequel on utilise un réacteur à membrane à liquide de mélange à retour complet, dont le fonctionnement est fondé sur la réaction liquide-liquide, pour conduire une réaction de nucléation rapide et ainsi obtenir le noyau magnétique nanométrique, puis on mélange ledit noyau avec la solution saline correspondante, on utilise le réacteur à membrane à liquide de mélange à retour complet pour conduire une réaction de nucléation rapide, on obtient alors de l'hydrotalcite qui contient le noyau magnétique et que l'on soumet à une calcination pour obtenir un oxyde composite à base solide dans lequel est enveloppé le noyau magnétique. Ce catalyseur se caractérise en ce que: il est d'une taille nanométrique, il présente une grande surface effective, ainsi qu'une activité et une sélectivité élevées dans la réaction catalytique. Etant donné que ce catalyseur est magnétique il peut être ramassé pour être récupéré et fortement dispersé dans un système de réaction par un champ magnétique extérieur. Ce catalyseur peut être utilisé pour conduire une réaction organique catalysée, telle que la synthèse d'éthers d'alcool, l'échange d'esters, la condensation d'aldéhyde-cétone, etc.
PCT/CN2003/000592 2002-07-23 2003-07-23 Catalyseur a base solide nanometrique magnetique et son procede de preparation WO2004009233A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU2003255081A AU2003255081A1 (en) 2002-07-23 2003-07-23 Magnetic nanometer solid base catalyst and its preparation method
US11/040,408 US7247598B2 (en) 2002-07-23 2005-01-21 Nano-scale magnetic solid base catalyst and its preparation method

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CN02125589.X 2002-07-23
CNB02125589XA CN1180881C (zh) 2002-07-23 2002-07-23 一种磁性纳米固体碱催化剂及其制备方法

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Cited By (3)

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US8114807B2 (en) 2010-03-05 2012-02-14 Cem Corporation Synthesis and use of intermetallic iron palladium nanoparticle compositions
CN103223345A (zh) * 2013-05-17 2013-07-31 北京化工大学 一种负载型Ni-In金属间化合物催化剂及其制备方法
CN105032431A (zh) * 2014-12-12 2015-11-11 北京恩泽福莱科技有限公司 一种磁性固体碱催化剂及其制备方法

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CN1317357C (zh) * 2005-01-27 2007-05-23 清华大学 一种固体碱催化剂及制备方法和应用
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CN102580663A (zh) * 2012-02-21 2012-07-18 上海大学 一种高磁性复合材料的制备方法及其应用
CN102847539B (zh) * 2012-09-29 2014-08-06 上海东升新材料有限公司 混晶固体碱组合催化剂及制备方法
CN103073063B (zh) * 2012-12-17 2014-11-12 沈阳化工大学 利用活性氧化镁为原料制备纳米铁酸镁的方法
CN109867589B (zh) * 2017-12-01 2022-04-19 万华化学集团股份有限公司 一种丙二醇单烷基醚的制备方法
CN107890871B (zh) * 2017-12-01 2020-04-28 东北石油大学 木质素磺酸盐催化解聚制取芳香基化合物的方法
CN108786830B (zh) * 2018-06-29 2020-11-03 中国科学院海洋研究所 一种镍钒复合氧化物模拟酶材料及其制备方法和用途

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8114807B2 (en) 2010-03-05 2012-02-14 Cem Corporation Synthesis and use of intermetallic iron palladium nanoparticle compositions
CN103223345A (zh) * 2013-05-17 2013-07-31 北京化工大学 一种负载型Ni-In金属间化合物催化剂及其制备方法
CN105032431A (zh) * 2014-12-12 2015-11-11 北京恩泽福莱科技有限公司 一种磁性固体碱催化剂及其制备方法

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